CN114315397A - Method for preparing fiber reinforced ceramic matrix composite - Google Patents
Method for preparing fiber reinforced ceramic matrix composite Download PDFInfo
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- CN114315397A CN114315397A CN202011055025.3A CN202011055025A CN114315397A CN 114315397 A CN114315397 A CN 114315397A CN 202011055025 A CN202011055025 A CN 202011055025A CN 114315397 A CN114315397 A CN 114315397A
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- 239000000835 fiber Substances 0.000 title claims abstract description 107
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 239000011159 matrix material Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 29
- 238000004804 winding Methods 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000005470 impregnation Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000007598 dipping method Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000003822 epoxy resin Substances 0.000 claims abstract description 4
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 239000003292 glue Substances 0.000 claims description 18
- 238000009835 boiling Methods 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 9
- 238000003754 machining Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052863 mullite Inorganic materials 0.000 claims description 4
- 238000007781 pre-processing Methods 0.000 claims 1
- 238000003980 solgel method Methods 0.000 abstract description 5
- 239000011153 ceramic matrix composite Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000000626 liquid-phase infiltration Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009730 filament winding Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
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Abstract
The invention relates to a method for preparing a fiber reinforced ceramic matrix composite. The method comprises the following steps: 1) carrying out fiber pretreatment to remove epoxy resin on the surface of the fiber; 2) dipping the pretreated fiber in the sol to obtain fully dipped fiber; 3) winding the dipped fibers on a core mold, and drying; 4) sequentially carrying out composite impregnation, drying, composite impregnation, drying and sintering on the dried sample piece; 5) and repeating the step 4) for a plurality of times to obtain the fiber reinforced ceramic matrix composite. The invention prepares the ceramic matrix composite material with high fiber volume content by combining the fiber winding process and the sol-gel method, not only can save time, improve mechanization and reduce production cost, but also can adjust the thermal mechanical property of the fiber reinforced ceramic matrix composite material by changing the fiber type, the ceramic matrix, the grain size distribution and the fiber orientation of the sol for impregnation and the winding mode.
Description
Technical Field
The invention relates to a novel method for preparing a fiber reinforced ceramic matrix composite, belonging to the field of composite preparation processes.
Background
The ceramic material has excellent performances of high melting point, low density, corrosion resistance, oxidation resistance, ablation resistance and the like, and is widely applied to special fields of aerospace, military industry and the like. However, the ceramic material has poor reliability in the use process due to large brittleness and poor plasticity and toughness, and the application range of the ceramic material is limited. Therefore, continuous fiber reinforced ceramic matrix composites have been developed by improving their properties through the use of continuous fiber toughening. The fiber reinforced ceramic matrix composite material overcomes the defect of brittle fracture of a ceramic material, and improves the thermal shock impact resistance of the material; meanwhile, the advantages of high temperature resistance, low expansion, low density and good thermal stability of the ceramic matrix are maintained.
The prior preparation method of the fiber reinforced ceramic matrix composite mainly comprises the following steps: slurry dip-hot pressing, chemical reaction, melt infiltration (dipping), sol-gel and precursor conversion. Most fiber reinforced ceramic matrix composites are prepared using a sol-gel process. However, the weaving of the fiber reinforcement of the fiber reinforced ceramic matrix composite material is mainly finished by hand at present, which not only increases the preparation period of the fiber reinforced ceramic matrix composite material, but also greatly limits the application range of the fiber reinforced ceramic matrix composite material due to the expensive weaving cost.
The development of filament winding technology has been over half a century, becoming one of the most important means in composite manufacturing processes. It has the highest mechanization degree and quite wide product range. The fiber winding product has the advantages of high specific strength, corrosion resistance, low cost, stable quality and the like, is easy to realize mechanization and automation, and has high production efficiency, so the fiber winding product is suitable for manufacturing large parts and repeatedly producing high-performance composite material structures. The fiber reinforced ceramic matrix composite material prepared by the fiber winding technology can reduce time cost and improve mechanization.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a novel method for preparing a fiber reinforced ceramic matrix composite.
The technical scheme adopted by the invention is as follows:
a method of making a fiber reinforced ceramic matrix composite, comprising the steps of:
1) carrying out fiber pretreatment to remove epoxy resin on the surface of the fiber;
2) dipping the pretreated fiber in the sol to obtain fully dipped fiber;
3) winding the dipped fibers on a core mold, and drying;
4) sequentially carrying out composite impregnation, drying, composite impregnation, drying and sintering on the dried sample piece;
5) and repeating the step 4) to obtain the fiber reinforced ceramic matrix composite.
Further, the pretreatment of step 1) comprises: boiling the fiber with acetone for 36-48h, then replacing with new acetone, continuing boiling for 12-24h, and finally airing for 3-4 days in an explosion-proof room.
Further, in the step 2), the pretreated fiber is soaked in sol for 2-5 hours, and the density of the sol is 1.20-1.38 g/cm3。
Further, the drying treatment of step 3) comprises: and (3) keeping the wound sample in an oven at the temperature of 80-120 ℃ for 12-24 h.
Further, step 4) comprises:
composite impregnation: putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24-36 h;
and (3) drying: after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80-120 ℃ for drying for 12-24 h;
composite impregnation: putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24-36 h;
and (3) drying: after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80-120 ℃ for drying for 12-24 h;
and (3) sintering: and (4) cooling, namely removing the core mold used for winding the sample piece, and then sintering at 600-800 ℃ for 45-90 min.
Further, the fibers are quartz fibers or alumina fibers; the sol is a silica sol, an alumina sol, or a mullite sol.
Further, the step 5) is repeated for a plurality of times until the mass change is lower than 1 percent, so as to obtain the fiber reinforced ceramic matrix composite material.
Furthermore, fiber reinforced ceramic matrix composite materials with different shapes are prepared by changing the fiber winding mode, the shape of the core mold and the fiber winding angle.
Further, the method also comprises the following machining steps: machining the sample obtained in the step 5) into a required shape.
The invention also provides a fiber reinforced ceramic matrix composite prepared according to the method.
The invention has the beneficial effects that:
(1) the invention provides a novel preparation process of a ceramic matrix composite, which is used for preparing the ceramic matrix composite with high fiber volume content by combining a fiber winding process and a sol-gel method. Compared with the slurry impregnation-hot pressing method, the chemical reaction method, the melt infiltration (impregnation) method, the sol-gel method, the precursor conversion method and other processes, the fiber winding-sol-gel process is adopted, so that the time can be saved, the mechanization is improved, the production cost is reduced, and the thermal mechanical property of the fiber reinforced ceramic matrix composite can be adjusted by changing the fiber type, the ceramic matrix, the particle size distribution and the fiber orientation of the sol for impregnation and the winding mode.
(2) By adjusting the particle size of the sol for impregnation, ceramic matrix composite materials with different fiber volume contents can be prepared.
(3) By selecting a suitable mandrel and by simple machining, a sample piece of a complex shape can be prepared.
Drawings
FIG. 1 is a process scheme of the method of making a fiber reinforced ceramic matrix composite of the present invention.
Detailed Description
The technical solution of the present invention is further described below with reference to examples.
The process route of the method for preparing the fiber reinforced ceramic matrix composite material is shown in figure 1, and the method comprises the following specific steps:
step 1, fiber pretreatment (fiber cleaning): the fiber surface will often have a thin layer of epoxy, the presence of which affects the interfacial bond strength of the fiber to the matrix material in the composite. It is desirable to select a suitable fiber pretreatment process to remove the epoxy resin from the fiber surface and minimize the impact on fiber strength. Boiling the fiber with acetone for 36-48h, then replacing with new acetone, continuing boiling for 12-24h, and finally airing for 3-4 days in an explosion-proof room.
Step 2, fiber impregnation: soaking the fiber treated in the step 1 in sol (the density of the sol is 1.20-1.38 g/cm)3) And 2-5h, obtaining the fully impregnated fiber.
Step 3, fiber winding: and winding the fibers onto the core mold through a winding machine according to a set winding program.
And 4, drying: and (4) keeping the wound sample piece in the step (3) in an oven at the temperature of 80-120 ℃ for 12-24 h.
Step 5, composite impregnation: putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the sol into a tank, pressurizing for 3.5-3.7 MPa, and maintaining the pressure for 24-36 h.
And 6, drying: and after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80-120 ℃ for drying for 12-24 h.
Step 7, composite impregnation: putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the sol into a tank, pressurizing for 3.5-3.7 MPa, and maintaining the pressure for 24-36 h.
And 8, drying: and after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80-120 ℃ for drying for 12-24 h.
Step 9, demolding and sintering: and (4) cooling, namely removing the core mold used for winding the sample piece, and then sintering at 600-800 ℃ for 45-90 min.
And step 10, repeating the composite impregnation, drying, composite impregnation, drying and sintering of the steps 5-9 until the mass change is lower than 1%.
Step 11, machining: the sample of step 10 is machined to the desired shape.
The fiber can be quartz fiber, alumina fiber, etc.
As the sol, silica sol, alumina sol, mullite sol, etc. can be used.
The fiber winding can be used for preparing composite materials with different shapes by changing the winding mode, the shape of the core mould and the winding angle.
The fiber impregnation in the step 2 has the effects that the sol is completely permeated into the fibers, the fiber is coated with the sol solution in the subsequent winding, the fiber abrasion can be reduced, the fiber arrangement parallelism is good, and the formed product has good air tightness; the subsequent composite impregnation has the function of improving the density of the product by multiple times of pressurized impregnation, so that the mechanical property of the composite material reaches the requirement of application.
Example 1:
boiling the B-type quartz fiber with acetone for 36h, then replacing with new acetone, continuing boiling for 12h, and finally airing for 3-4 days in an explosion-proof room; soaking the cleaned quartz fiber in a solution with a density of 1.20g/cm3Obtaining fully impregnated fiber after 2 hours in the silica sol; winding the fibers on the circular truncated cone core die through a winding machine according to a set winding program; keeping the wound sample piece in an oven at 80 ℃ for 12 h; putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the silica sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24 hours; after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80 ℃ for drying for 12 hours; putting the dried sample piece into a glue injection tankThe density is 1.25 to 1.32g/cm3Injecting the silica sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24 hours; cooling, namely removing a core mold used for winding the sample piece, and then sintering at 600 ℃; circulating, dipping in glue for 8 times, and sintering after even number of times of dipping to obtain cylindrical ring with density of 1.65g/cm3。
Example 2:
boiling Nextel720 alumina fiber with acetone for 36h, then replacing with new acetone, continuing boiling for 12h, and finally airing for 3-4 days in an explosion-proof room; the cleaned alumina fiber is dipped in the solution with the density of 1.38g/cm3Obtaining fully impregnated fiber after 2 hours in the silica sol; winding the fiber on the plate-shaped core mold through a winding machine according to a set winding program; keeping the wound sample piece in an oven at 100 ℃ for 12 h; putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the silica sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24 hours; after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80 ℃ for drying for 12 hours; putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the silica sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24 hours; cooling, namely removing a core mold used for winding the sample piece, and then sintering at 600 ℃; circulating, dipping in glue for 8 times, sintering after even number of times of dipping in glue to obtain square annular column, and machining to obtain alumina fiber reinforced ceramic matrix composite plate with density of 2.2g/cm3。
Example 3:
boiling Nextel550 alumina fiber with acetone for 36h, then replacing with new acetone, continuing boiling for 12h, and finally airing for 3-4 days in an explosion-proof room; the cleaned alumina fiber is dipped in the solution with the density of 1.30g/cm3Obtaining fully impregnated fiber after 2 hours in the mullite sol; modifying the winding direction according to a set winding program, winding the fibers on a cylindrical core mold through a winding machine, wherein the winding shape is a circular tube with holes; keeping the wound sample piece in an oven at 80 ℃ for 12 h; putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the aluminum sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24 hours; after the pressure maintaining is finishedSending the sample piece into a 100 ℃ oven for drying for 12 hours; putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the aluminum sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24 hours; cooling, namely removing a core mold used for winding the sample piece, and then sintering at 600 ℃; circulating, dipping in glue for 10 times, sintering after even number of times of dipping in glue to obtain circular pipe with holes and density of 2.70g/cm3。
The foregoing disclosure of the specific embodiments of the present invention and the accompanying drawings is directed to an understanding of the present invention and its implementation, and it will be appreciated by those skilled in the art that various alternatives, modifications, and variations may be made without departing from the spirit and scope of the invention. The present invention should not be limited to the disclosure of the embodiments and drawings in the specification, and the scope of the present invention is defined by the scope of the claims.
Claims (10)
1. A method of making a fiber reinforced ceramic matrix composite, comprising the steps of:
1) carrying out fiber pretreatment to remove epoxy resin on the surface of the fiber;
2) dipping the pretreated fiber in the sol to obtain fully dipped fiber;
3) winding the dipped fibers on a core mold, and drying;
4) sequentially carrying out composite impregnation, drying, composite impregnation, drying and sintering on the dried sample piece;
5) and repeating the step 4) to obtain the fiber reinforced ceramic matrix composite.
2. The method of claim 1, wherein the pre-processing of step 1) comprises: boiling the fiber with acetone for 36-48h, then replacing with new acetone, continuing boiling for 12-24h, and finally airing for 3-4 days in an explosion-proof room.
3. The method according to claim 1, wherein step 2) is carried out by dipping the pretreated fibers in a sol for 2-5h, said sol being obtainedThe density of the glue is 1.20-1.38 g/cm3。
4. The method according to claim 1, wherein the drying process of step 3) comprises: and (3) keeping the wound sample in an oven at the temperature of 80-120 ℃ for 12-24 h.
5. The method of claim 1, wherein step 4) comprises:
composite impregnation: putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24-36 h;
and (3) drying: after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80-120 ℃ for drying for 12-24 h;
composite impregnation: putting the dried sample piece into a glue injection tank, and setting the density to be 1.25-1.32 g/cm3Injecting the sol into a tank, pressurizing at 3.5-3.7 MPa, and maintaining the pressure for 24-36 h;
and (3) drying: after the pressure maintaining is finished, the sample piece is sent into an oven with the temperature of 80-120 ℃ for drying for 12-24 h;
and (3) sintering: and (4) cooling, namely removing the core mold used for winding the sample piece, and then sintering at 600-800 ℃ for 45-90 min.
6. The method of claim 1, wherein the fibers are quartz fibers or alumina fibers; the sol is a silica sol, an alumina sol, or a mullite sol.
7. The method according to claim 1, wherein step 5) is repeated step 4) a plurality of times until the mass change is less than 1% to obtain the fiber reinforced ceramic matrix composite material.
8. The method of claim 1, wherein different shapes of fiber reinforced ceramic matrix composites are produced by varying the fiber winding pattern, the shape of the mandrel, and the fiber winding angle.
9. The method according to any one of claims 1 to 8, further comprising the step of machining: machining the sample obtained in the step 5) into a required shape.
10. A fiber reinforced ceramic matrix composite prepared according to the method of any one of claims 1-9.
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| CN116003147A (en) * | 2023-01-09 | 2023-04-25 | 山东工业陶瓷研究设计院有限公司 | Reinforced ceramic fiber filter material and preparation method thereof |
| CN116354736A (en) * | 2023-03-27 | 2023-06-30 | 中国人民解放军国防科技大学 | Preparation method of fiber reinforced alumina ceramic matrix composite |
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Application publication date: 20220412 |